CN106732445A - A kind of silica modified heavy metal wastewater thereby adsorbent and preparation method thereof - Google Patents
A kind of silica modified heavy metal wastewater thereby adsorbent and preparation method thereof Download PDFInfo
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- CN106732445A CN106732445A CN201611078184.9A CN201611078184A CN106732445A CN 106732445 A CN106732445 A CN 106732445A CN 201611078184 A CN201611078184 A CN 201611078184A CN 106732445 A CN106732445 A CN 106732445A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/265—Synthetic macromolecular compounds modified or post-treated polymers
- B01J20/267—Cross-linked polymers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
- C02F2101/22—Chromium or chromium compounds, e.g. chromates
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Abstract
The invention discloses a kind of silica modified heavy metal wastewater thereby adsorbent and preparation method thereof, matched by weight by following components and constituted：9~32 parts of silica 1,13~26 parts of tetraethyl orthosilicate, 13~28 parts of 3 aminopropyl triethoxysilane, 12~25 parts of salicylide, 8~17 parts of dichloromethane, 8~19 parts of absolute ethyl alcohol, 9~17 parts of sodium acid carbonate, 7~19 parts of copper nitrate, 13~22 parts of maleic anhydride, 12~25 parts of glutaraldehyde.(1) silica modified heavy metal wastewater thereby adsorbent of the present invention has the mesoporous silicon oxide of the high-sequential of chelation, and with bigger serface, pore passage structure is regular, and aperture is big and adjustable, high-adsorption-capacity；(2) absorption of silica modified heavy metal wastewater thereby adsorbent heavy metal ion of the present invention has high selectivity, improves the validity of the heavy metal absorption in low concentration pollution.
Description
Technical field
The invention belongs to field of environment protection, it is related to a kind of heavy metal in water recovery technique, more particularly to a kind of titanium dioxide
Heavy metal wastewater thereby adsorbent of Si modification and preparation method thereof.
Background technology
Heavy metal wastewater thereby is mainly derived from mining, steel and non-ferrous metal metallurgy, metal material and metallic article
Processing and use process, such as mine hole internal drainage, waste-rock yard drench immersion, mill tailings draining, steel plant pickling draining, have
Non-ferrous metal smeltery dedusting draining, the acid washing water of Non-ferrous Metals Processing Factory, Electroplate Factory's plating piece washings and battery, paint, face
The industry such as material, rubber, plastics, agricultural chemicals, chemical fertilizer, leather.Wherein mining and smelting are topmost pollution sources.Weight in waste water
The species of metal, content and existing forms are changed greatly with different production industries
Comprehensive domestic and foreign literature, the heavy metal wastewater thereby species for summarizing various production activity discharges is as follows：Mining and smelting row
Industry primary discharge copper, lead, zinc, cadmium, mercury etc.；Electroplating industry primary discharge Cr VI, copper, zinc, nickel, cadmium, tin etc.；Cell row owner
Discharge lead, zinc, mercury, cadmium etc.；Pigment industry primary discharge mercury, Cr VI, lead, cadmium, arsenic, zinc etc.；Paint store industry primary discharge
Cadmium, lead, Cr VI etc.；Primary discharge copper, zinc, Cr VI etc. in the building-up process of rubber；Plastic industry primary discharge lead, arsenic,
Mercury etc.；Agricultural chemicals, fertilizer industry primary discharge arsenic；Leather industry primary discharge Cr VI.The heavy metal of these discharges is primarily present
In the waste water of industrial discharge and the filtrate of solid waste landfills.Due to its shape can only be changed after in heavy metals emission to environment
State is transferred, dilutes, accumulating in vivo, and can not be degraded, thus endangers larger.
The harm of heavy metal, shows specific to different heavy metal ion and differs again.For example, heavy metal Hg is savings property poison
Thing, in addition to chronic and acute poisoning, also carcinogenic and mutagenic effect, Japanese Mad Hatter's disease is because methyl mercury is in people and animals' brain
Mouth caused by middle accumulation；Cadmium pollution can make one the calcareous alienation of bone, fracture occur, be commonly called as " itai-itai " be chronic cadium poisoning most
Typical example；The harm of chromium be mainly shown as intoxicating effect, stimulation, cumulative function, allergy, carcinogenesis and
Mutagenesis, the harm to nerve cell is maximum, and hexavalent chromium compound is then possible to cause many acute diseases, such as hepatic injury,
Ulcer, perforation of nasal septum and breathing cancer；Lead is a kind of heavy metal element with neurotoxicity, lead major determinant marrow hemopoiesis system
System and nervous system, trigger anemia, nervous function imbalance and injury of kidney, and children are caused with the infringement of brain；Copper is once by stomach
Intestinal absorption, will enter blood, muscle, liver and brain, cause a series of illnesss such as gastrointestinal disease, injury of kidney, anaemia；Zinc
Though one of the essential trace elements of the human body, but if eating the food excess of reinforcing zinc, it will cause zinc poisoning.Therefore, weight
Metallic pollution oneself turn into and be related to the great environmental problem of human health and life.
Absorption method is the method that Pollutants in Wastewater is removed using porous sorbing material.Preferable adsorbent should possess
Following features, i.e. material source are extensive, cheap, high adsorption capacity, adsorptive selectivity are good, adsorption equilibrium concentration is low, machinery
Intensity is good, stable chemical nature, regenerating easily and utilization.General industry adsorbent is difficult while meeting wanting for above-mentioned 8 aspects
Ask, therefore, different adsorbents should be selected according to different occasions.
At present, the adsorbent (comprising commercial Application and laboratory research) applied in wastewater treatment has charcoal class adsorbent, corruption
Grow acids adsorbent, mineral adsorbent, polymeric sorbent, biological adsorption agent, industrial waste adsorbent etc..It is earliest as application
One of most wide adsorbent, activated carbon has general applicability, but its price is costly.Thus, find/exploitation it is cheap and easy to get and
One of the sorbing material of recoverable, the study hotspot as current water process.The mechanism of humic acid Adsorption of Heavy Metals be from
Son is exchanged and chelation, and adsorption effect is good, but the desorption of heavy metal ion is more difficult.After being eluted with EDTA, in eluent
The separation of heavy metal is also a problem.Mineral adsorbent have the advantages that it is cheap, but except bentonite, modified zeolite etc.
Outside a few, its adsorption capacity is totally relatively low, and after very years of researches, most researchs remain in reality
Test the room stage.Organic polymer performance of the adsorbent is good, and its limitation is that material is easily oxidized, corrodes, and mechanical strength is poor, should
It is restricted with occasion.Because the culture microorganism cycle is long, low yield, and plant adsorbent overall adsorption capacity is smaller, thus
The research of biological adsorption agent at present more rests on laboratory stage.
To sum up, the adsorbent species currently studied are numerous, but adsorption capacity between various adsorbents is uneven,
The use cost of material also height.Although mineral adsorbent and industry, agricultural wastes source are extensively, Environmental compatibility is good,
But adsorption capacity is relatively low；The natural macromolecule adsorbents such as shitosan, cellulose, absorption property is good, and material is environmentally friendly low in itself
Carbon, but inoxidizability and biological stability are poor under complicated condition of water quality；Microbial adsorbent has strain source wide, treatment
Efficiency high, the advantages of can reclaim heavy metal, but in water is in often discrete state due to thalline, it is necessary to first carry out immobilization side
Can be used, and the toxigenic capacity of thalline is high, makes its research still many in laboratory stage.Activated carbon and ion exchange resin are
Industrially apply two kinds of more materials.But traditional charcoal absorption capacity is relatively low, is compared with many adsorbents and do not possessed
Advantage on cost and performance, by modified, adsorption capacity has a distinct increment.And ion exchange resin is easily received due to resin
Pollution or oxidation deactivation, application scenario are subject to larger limitation.Therefore, sorbing material new and effective, applied widely is developed
One of key as absorption method success application.
The content of the invention
Present invention solves the technical problem that：In order to overcome the defect of prior art, a kind of height with chelation is obtained
The orderly mesoporous silicon oxide of degree, with bigger serface, pore passage structure is regular, and aperture is big and adjustable, and high-adsorption-capacity etc. is excellent
The adsorbent of point, the invention provides a kind of silica modified heavy metal wastewater thereby adsorbent and preparation method thereof.
Technical scheme：A kind of silica modified heavy metal wastewater thereby adsorbent, is matched by weight by following components
Composition：9~32 parts of silica 1,13~26 parts of tetraethyl orthosilicate, 13~28 parts of 3- aminopropyl triethoxysilanes, bigcatkin willow
12~25 parts of aldehyde, 8~17 parts of dichloromethane, 8~19 parts of absolute ethyl alcohol, 9~17 parts of sodium acid carbonate, 7~19 parts of copper nitrate, Malaysia
13~22 parts of acid anhydrides, 12~25 parts of glutaraldehyde.
Preferably, the silica modified heavy metal wastewater thereby adsorbent is by following components proportioning group by weight
Into：26 parts of silica, 21 parts of tetraethyl orthosilicate, 22 parts of 3- aminopropyl triethoxysilanes, 19 parts of salicylide, dichloromethane
13 parts, 14 parts of absolute ethyl alcohol, 15 parts of sodium acid carbonate, 16 parts of copper nitrate, 16 parts of maleic anhydride, 19 parts of glutaraldehyde.
A kind of preparation method of silica modified heavy metal wastewater thereby adsorbent, comprises the steps of：
(1) prepared by adsorbent matrix：After tetraethyl orthosilicate, 3- aminopropyl triethoxysilanes and salicylide are mixed,
Attrition grinding, is 90~120 mesh to particle diameter, is placed in baking oven 90~110 DEG C and processes 65~100 minutes；
(2) it is modified for the first time：By in silica addition adsorbent matrix, it is placed in crucible and heats, 7 is added dropwise in heating
~22% sulfuric acid solution, stops heating afterwards in the pasty state；
(3) it is modified for second：During dichloromethane and absolute ethyl alcohol are added through adsorbent matrix modified for the first time, mix
After closing uniformly, 30~45 DEG C are reacted 1~3.5 hour, and crucible continues to heat, and stopping of being volatilized completely to moisture is heated；
(4) cross-linking reaction：To addition sodium acid carbonate, copper nitrate, maleic anhydride in second modified adsorbent matrix
And glutaraldehyde, 4~8 DEG C are reacted 30~80 minutes；
(5) finished product：Crosslinked reacted product is placed in baking oven, and 90~110 DEG C of reactions can be prepared by for 1~3.5 hour.
Preferably, prepared by step (1) adsorbent matrix：By tetraethyl orthosilicate, 3- aminopropyl triethoxysilanes and water
After the mixing of poplar aldehyde, attrition grinding is 110 mesh to particle diameter, is placed in baking oven 102 DEG C and processes 85 minutes.
Preferably, step (2) is modified for the first time：By in silica addition adsorbent matrix, it is placed in crucible and heats, side
Heating side is added dropwise 16% sulfuric acid solution, stops heating afterwards in the pasty state.
Preferably, step (3) is modified for second：Dichloromethane and absolute ethyl alcohol are added through absorption modified for the first time
In agent matrix, after being well mixed, 42 DEG C are reacted 2.5 hours, and crucible continues to heat, stopping heating of being volatilized completely to moisture.
Preferably, step (4) cross-linking reaction：To addition sodium acid carbonate, nitric acid in second modified adsorbent matrix
Copper, maleic anhydride and glutaraldehyde, 6 DEG C are reacted 60 minutes.
Preferably, step (5) finished product：Crosslinked reacted product is placed in baking oven, and 102 DEG C of reactions 3 hours can system
.
Beneficial effect：(1) silica modified heavy metal wastewater thereby adsorbent of the present invention has the height of chelation
The orderly mesoporous silicon oxide of degree, with bigger serface, pore passage structure is regular, and aperture is big and adjustable, high-adsorption-capacity；(2)
The absorption of silica modified heavy metal wastewater thereby adsorbent heavy metal ion of the present invention has high selectivity, improves
The validity of heavy metal absorption in low concentration pollution.
Specific embodiment
Embodiment 1
A kind of silica modified heavy metal wastewater thereby adsorbent, is matched and constituted by weight by following components：Dioxy
19 parts of SiClx, 13 parts of tetraethyl orthosilicate, 13 parts of 3- aminopropyl triethoxysilanes, 12 parts of salicylide, 8 parts of dichloromethane, nothing
8 parts of water-ethanol, 9 parts of sodium acid carbonate, 7 parts of copper nitrate, 13 parts of maleic anhydride, 12 parts of glutaraldehyde.
A kind of preparation method of silica modified heavy metal wastewater thereby adsorbent, comprises the steps of：
(1) prepared by adsorbent matrix：After tetraethyl orthosilicate, 3- aminopropyl triethoxysilanes and salicylide are mixed,
Attrition grinding, is 90 mesh to particle diameter, is placed in baking oven 90 DEG C and processes 65 minutes；
(2) it is modified for the first time：By in silica addition adsorbent matrix, it is placed in crucible and heats, is added dropwise in heating
7% sulfuric acid solution, stops heating afterwards in the pasty state；
(3) it is modified for second：During dichloromethane and absolute ethyl alcohol are added through adsorbent matrix modified for the first time, mix
After closing uniformly, 30 DEG C are reacted 1 hour, and crucible continues to heat, and stopping of being volatilized completely to moisture is heated；
(4) cross-linking reaction：To addition sodium acid carbonate, copper nitrate, maleic anhydride in second modified adsorbent matrix
And glutaraldehyde, 4 DEG C are reacted 30 minutes；
(5) finished product：Crosslinked reacted product is placed in baking oven, and 90 DEG C of reactions can be prepared by for 1 hour.
Embodiment 2
A kind of silica modified heavy metal wastewater thereby adsorbent, is matched and constituted by weight by following components：Dioxy
26 parts of SiClx, 21 parts of tetraethyl orthosilicate, 22 parts of 3- aminopropyl triethoxysilanes, 19 parts of salicylide, 13 parts of dichloromethane, nothing
14 parts of water-ethanol, 15 parts of sodium acid carbonate, 16 parts of copper nitrate, 16 parts of maleic anhydride, 19 parts of glutaraldehyde.
A kind of preparation method of silica modified heavy metal wastewater thereby adsorbent, comprises the steps of：
(1) prepared by adsorbent matrix：After tetraethyl orthosilicate, 3- aminopropyl triethoxysilanes and salicylide are mixed,
Attrition grinding, is 110 mesh to particle diameter, is placed in baking oven 102 DEG C and processes 85 minutes；
(2) it is modified for the first time：By in silica addition adsorbent matrix, it is placed in crucible and heats, is added dropwise in heating
16% sulfuric acid solution, stops heating afterwards in the pasty state；
(3) it is modified for second：During dichloromethane and absolute ethyl alcohol are added through adsorbent matrix modified for the first time, mix
After closing uniformly, 42 DEG C are reacted 2.5 hours, and crucible continues to heat, and stopping of being volatilized completely to moisture is heated；
(4) cross-linking reaction：To addition sodium acid carbonate, copper nitrate, maleic anhydride in second modified adsorbent matrix
And glutaraldehyde, 6 DEG C are reacted 60 minutes；
(5) finished product：Crosslinked reacted product is placed in baking oven, and 102 DEG C of reactions can be prepared by for 3 hours.
Embodiment 3
A kind of silica modified heavy metal wastewater thereby adsorbent, is matched and constituted by weight by following components：Dioxy
32 parts of SiClx, 26 parts of tetraethyl orthosilicate, 28 parts of 3- aminopropyl triethoxysilanes, 25 parts of salicylide, 17 parts of dichloromethane, nothing
19 parts of water-ethanol, 17 parts of sodium acid carbonate, 19 parts of copper nitrate, 22 parts of maleic anhydride, 25 parts of glutaraldehyde.
A kind of preparation method of silica modified heavy metal wastewater thereby adsorbent, comprises the steps of：
(1) prepared by adsorbent matrix：After tetraethyl orthosilicate, 3- aminopropyl triethoxysilanes and salicylide are mixed,
Attrition grinding, is 120 mesh to particle diameter, is placed in baking oven 110 DEG C and processes 100 minutes；
(2) it is modified for the first time：By in silica addition adsorbent matrix, it is placed in crucible and heats, is added dropwise in heating
22% sulfuric acid solution, stops heating afterwards in the pasty state；
(3) it is modified for second：During dichloromethane and absolute ethyl alcohol are added through adsorbent matrix modified for the first time, mix
After closing uniformly, 45 DEG C are reacted 3.5 hours, and crucible continues to heat, and stopping of being volatilized completely to moisture is heated；
(4) cross-linking reaction：To addition sodium acid carbonate, copper nitrate, maleic anhydride in second modified adsorbent matrix
And glutaraldehyde, 8 DEG C are reacted 80 minutes；
(5) finished product：Crosslinked reacted product is placed in baking oven, and 110 DEG C of reactions can be prepared by for 3.5 hours.
The performance of the silica modified heavy metal wastewater thereby adsorbent prepared to embodiment 1~3 is detected, tied
It is really as shown in the table：
| Embodiment 1 | Embodiment 2 | Embodiment 3 | |
| Pb clearances/% | 98.1 | 99.9 | 99.7 |
| Cu clearances/% | 97.9 | 99.8 | 99.5 |
| Ni clearances/% | 46.8 | 69.7 | 62.5 |
| Zn clearances/% | 49.2 | 65.2 | 52.3 |
| Mn clearances/% | 23.4 | 39.8 | 29.5 |
| Cd clearances/% | 37.2 | 59.2 | 52.3 |
Claims (8)
1. a kind of silica modified heavy metal wastewater thereby adsorbent, it is characterised in that matched by weight by following components
Composition：9~32 parts of silica 1,13~26 parts of tetraethyl orthosilicate, 13~28 parts of 3- aminopropyl triethoxysilanes, bigcatkin willow
12~25 parts of aldehyde, 8~17 parts of dichloromethane, 8~19 parts of absolute ethyl alcohol, 9~17 parts of sodium acid carbonate, 7~19 parts of copper nitrate, Malaysia
13~22 parts of acid anhydrides, 12~25 parts of glutaraldehyde.
2. a kind of silica modified heavy metal wastewater thereby adsorbent according to claim 1, it is characterised in that by following
Component matches composition by weight：26 parts of silica, 21 parts of tetraethyl orthosilicate, 3- aminopropyl triethoxysilanes 22
Part, 19 parts of salicylide, 13 parts of dichloromethane, 14 parts of absolute ethyl alcohol, 15 parts of sodium acid carbonate, 16 parts of copper nitrate, 16 parts of maleic anhydride,
19 parts of glutaraldehyde.
3. the preparation method of a kind of silica modified heavy metal wastewater thereby adsorbent described in claim 1, it is characterised in that
Comprise the steps of：
(1) prepared by adsorbent matrix：After tetraethyl orthosilicate, 3- aminopropyl triethoxysilanes and salicylide are mixed, crush
Grinding, is 90~120 mesh to particle diameter, is placed in baking oven 90~110 DEG C and processes 65~100 minutes；
(2) it is modified for the first time：During silica added into adsorbent matrix, it is placed in crucible and heats, it is added dropwise 7 in heating~
22% sulfuric acid solution, stops heating afterwards in the pasty state；
(3) it is modified for second：Dichloromethane and absolute ethyl alcohol are added through in adsorbent matrix modified for the first time, mixing is equal
After even, 30~45 DEG C are reacted 1~3.5 hour, and crucible continues to heat, stopping heating of being volatilized completely to moisture；
(4) cross-linking reaction：To addition sodium acid carbonate, copper nitrate, maleic anhydride and penta in second modified adsorbent matrix
Dialdehyde, 4~8 DEG C are reacted 30~80 minutes；
(5) finished product：Crosslinked reacted product is placed in baking oven, and 90~110 DEG C of reactions can be prepared by for 1~3.5 hour.
4. a kind of preparation method of silica modified heavy metal wastewater thereby adsorbent according to claim 3, its feature
It is prepared by step (1) adsorbent matrix：After tetraethyl orthosilicate, 3- aminopropyl triethoxysilanes and salicylide are mixed,
Attrition grinding, is 110 mesh to particle diameter, is placed in baking oven 102 DEG C and processes 85 minutes.
5. a kind of preparation method of silica modified heavy metal wastewater thereby adsorbent according to claim 3, its feature
It is that step (2) is modified for the first time：By in silica addition adsorbent matrix, it is placed in crucible and heats, is added dropwise in heating
16% sulfuric acid solution, stops heating afterwards in the pasty state.
6. a kind of preparation method of silica modified heavy metal wastewater thereby adsorbent according to claim 3, its feature
It is that step (3) is modified for second：During dichloromethane and absolute ethyl alcohol are added through adsorbent matrix modified for the first time,
After well mixed, 42 DEG C are reacted 2.5 hours, and crucible continues to heat, stopping heating of being volatilized completely to moisture.
7. a kind of preparation method of silica modified heavy metal wastewater thereby adsorbent according to claim 3, its feature
It is, step (4) cross-linking reaction：To addition sodium acid carbonate, copper nitrate, maleic anhydride in second modified adsorbent matrix
And glutaraldehyde, 6 DEG C are reacted 60 minutes.
8. a kind of preparation method of silica modified heavy metal wastewater thereby adsorbent according to claim 3, its feature
It is, step (5) finished product：Crosslinked reacted product is placed in baking oven, and 102 DEG C of reactions can be prepared by for 3 hours.
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